Process of manufacturing distillable spirits by fermentation



April 18, 1933. s. D. WELLS 1,904,589

PROCESS OF MAUFACTURING DISTILLABLE SPIRITS BY FERMENTATION Filed June 1'7, 1931 6000 C C' CULTL/Z' /A/ GLASS S11/manioc Sydney We ZZ@ lat'ented Apr. 1&'1933 SIDNEY D. F PORT RDW, WISO() l rnocnss or aci-name ms'rrnnannn smrrs BY Application led June 17, 1981. Serial Re. 545,125.

This invention relates to the production of alcohols by fermentation which is carried on under conditions particularly conducive to vigorous action in a mash rich in carbohydrate and nitrogenous matter.

The present invention is a continuation in part of my conding application Serial No. 190,556, led ay 11, 1927, which issued as Patent No. 1,823,014.

The invention is particularly directed to an improvement of the mash material and conditions ,of fermentation to effect a large yield of fermented product, Whether it be alcohol, ketones or an aldehyde or other product obtainable by fermentation. This improvement is brought about by using a certain material as the basis of the bulk of the mash. This particular material is the spent cooking liquor remaining after brous vegetable material has been cooked with certain particular mild cooking'agents and the liquor has a neutral or vonly slightly acid reaction. Y

Y In my Patent No. 1,823,014 I have described a process of alcoholic fermentation using a mash derived from fibrous plant material, in which the plant material is cooked with certain mild cooking agents, such as sodium carbon-ate, Vsodium sulphite, sodium sulphide or the like, or mixtures of the same. vBy the process of the present invention, I contemplate the'use of these same mild cooking agents, but intend particularly to stress the feature of having present in the soaking, steeping or cookin solution an amount of caustic alkali. e presence of a small amount of this caustic alkali, such as the caustic soda present in soda ash, is of great value linity of the treating solution whilerat the same time being of suicient dilution to keep the'strength of the cooking liquor suiciently low to secure satisfactory results on the mash.

In cooking strawl or other fibrous plant material with mild cooking agents such as sodium carbonate, sodium sulphite, sodium sulphide and the like or -mixtures of the same for the production of paper pulp the s nt cooking liquors are neutral or onlyslightly acid or may be readily rendered only slightly in maintaining the proper degree of a1ka' from acid` and they are rich in carbohydrate and nitrogenous vegetable material. They are. consequently capable of supporting numerous bacterial, fungal and other growths which produce various materials such as aliphatic alcohols, acids, aldehydes, ketones, esters, carbon dioxide, hydrogen, ammonia, and others, depending on what garticular growth or growths predominate. y using pure cul tures and sterilized liquor and equipment, the number of products produced ma be limited closely to the particular ones esired, and thus results are possible' similar to those obtained from the treatment of starchy material in the production of grain alcohol, acetic acid, and others.

Itisoftheutmostim rtaneethatthematerial of the 'mash used 1n thisl present invention have the qualities, ingredients and general charac 'cs herein dei'ned. Astrong cooking liquor such as that from caustic processes is not suitable, nor is the ar. containing material resultant of the so-ca ed sulphite cooln'ng satisfactory for the purposes of the present invention.

On the attached drawing thereis illustrated a flow sheet showing t e several steps of Ythe present invention. According to this chart, the microorganism is specified as 'loshlz'wn acetobutylcwn. Another satisfactory bacterium i's identified as B. Granula- :bacter pectovmwm. A culture is prepared of the `desired bacteria and the s res Vare developedon soil, then shocked. est tube cultures are prepared and about six thousand ec. are prepared in glass. A. fty' galion culture 1s prepared with sterilized cooking liquor of the type used in this invention an this quantity a one thousand galion culture is prepared with liquor. 'Separately from the foregoing, a large amount of cooking liquor in batches of ap vroximately fifty thousand gallons is first sterilized andthen p vthrough coolers and then placed in the fel-inenting apparatus and at this stage, the above mentioned one thousand gallon culture is incorporated and the fermenting conducted in the'sterilizedand cooled mash thus consistingof the cook-A s ing liquor. From the formentera the liquid 10 containin the desired products is drawn od' or otherwise separated and led to a reservoir from which. it is conducted to stills from which a crude spirit is obtainable. The crude spirit is subsequently fractionated and acetone alcohol and butanol and various mixed fractions are obtainable. The alcohol is ethyl alcohol or the product may be otherwise specifically predetermined, asjdesired. Other incidental products `are obtainable during the fermentation and subsequent treatment. At the .fermenters the driven oil includes carbon dioxide and ydrogen, both of which can be used. From the stills a i5 soda liquor is obtained and this can be converted to soda ash by subsequent treatment in evaporators, incinerators and leachin cells.

An-example in the production of t e solvents butanol, acetone, and cth l alcohol will 2@ be understood from the following procedure.

` The black liquor obtained from washin cereal straw cooked with a solution of s 'um carbonate and sulphur is sterilized aand inoculated with a culture of Uloadewn acel 915 tobutylzc'um (Wez'zwmnn) and allowed to ferment at a temperature of 98 F. until the ,evolution of gas ceases, a period of approximately sixty hours. The solution is then passed through continuous stills which yield a crude spirit consistin of about ity percent mixture of butano acetone, and ethyl alcohol in water. TheseV constituents are separated in fractionating columns as above outlined in connection withfthe accompanying drawing.

One of the important phases of this invention is the preparation of a nutrient solution capable of sustaining yeast and bacteria.v for the production of organic substances. Thus the invention may in part be considered directed toward the treatment of straw or other vegetable material for the production of the necessary nutrient solution.` In preparing the mash, thus consisting of the cooking liqcc uor specificall defined or of wash water resultant of was g fibrous plant material after such cooking, straw may be treated with a milk of lime solutionv containing approximately ten percent of the weight of the straw CaO or it may be treated with a solution containing five percent of its weight NMCO, and one-half rcent S, or it may be treated with asolut1on containing seven percent NagCOa and one and one-half percent NazSOs, or it may be treated with a so lution containin three percent NaGH and two percent Na2 In each case it is-cookedl in a digestor at a temperature of about 250 F. for ten hours. The contents are then 30 emptied and the soluble .matter'washe'd from the residue. Where milk of lime is used it is necessa to neutralize the liquors obtained with HZS 4 or NaHSO,L or some other acid or acid salt with a di-valent or tri-valent acid l5 until the right hydrogen ion :concentration iis -from the cooking of wood have addition of acids or acid salts prior to the adi Lacasse obtained moet lavorable to the qrrowtli el yeast or whatever bacteria is u ln the case of coohn solutions in which sodium salts are used t e liquors obtained are usually approximately theright hydrogen ion concentration and may be made exactly so by means of acid or alkali. The treatment of the solution with yeast and the distillation of the products obtained are carried on according to the methods hown to those versed in the art. Where brous ve etable material is used, the residue obtained m the digestion mentioned above may be used in the manufacture of paper, paperboard or other brous products `according to methods hewnto those versed in the art.

ln a somewhat dierent treatment, straw may be Itreated with a solution containing from live to ten rcent of its weight in soda ash or in a solutwn containing from four'to ten percent of its weight of caustic soda. The other cookin conditions would be the same as above speci ed. Different amounts require diderent cooking conditions. The amount of coongl reagent may be varied greatly and depends on the relative value of the solvents obtainable from the spent cooking liquor and the straw-board obtained from the brous residue. lt has been noticed that the greater the amount of cooking material and the more severe the cooking conditions there results a correspondingly greater amount of straw matter dissolved in the liquor and the smaller the amount of fibrous residue.

le is important thatl the @solang step be 1 alkaline or a neutral digestion and in this feature, the present process is to be (liderantiated from fermentation of materials reuiring the presence of sugar, as Vfor example, t ose in which waste sulphlte liqggers resultant n used andv the fermentation is confined probably solely to sugars which can exist in an acid di 'om In the present mash there is probab y little or no sugar. The substances which render the liquor of the mash of the present invention particularly important for 'fermentation purposesare peculiar in that these materials are not derived from cellulose but actually occur with the cellulose in the plant and are obtained without any breaking down of the cellulose to sugar as is the condition occurring in the bi-sulphite process.

The waste liquors obtained from the mild of various straws, bagasse, bamboo, grasses andthe like are particularly suitable to bacterial growth. Should there be slight alkalinity, this can be counteracted by the 12. ff dition of the ferment tothe mash. Suitable examples of acidifying materials are sulo phuric acid, phosphoric acid, carbonic acid,

' sodium acid sulphate or calcium mono phosphate and these materials maybe used to 1:

hemi-celluloses and pentosans, normally found in straw and similar vegetation, andalso albuminous matter and mucilaginous substances similar to pectin. All of these materials differ considerably from sugars, and such other carbohydrates obtainable from severe cooking treatment of wood such as referred to hereinbefore as providing a strong acid or strong alkali treatment. f

The conditions prescribed in the foregoing for the cooking reagent are typical, but the present process is not limited to the particuylar cooking materials, mentioned. l Quite a wide` variation of cooking materials may be used. .However, it is of major .importance that the cook be a mild cook and that the action be terminated before the vegetable material is pulped and approximately as soon as it, is softened, as contrasted to being pulped Thus the cooking material is substantially the same kind and strength of pecking reagent as I have defined for use for the treatment of vegetable fibrous material for the production of gulp by two stages including rst a mild coo ng to effect softening as contrasted to pulping and secondly, a treatment of the softened fibers by mechanical means to effect their separation and all of which features have been dened in my applications for 'patent for the production of pulp, Serial Nos. 38,354, filed June 19, 1925 and 49,461, filed August l0, 1925.

ii claim:

l. The process 'of manufacturing distillable spirits by fermentation which process comprises ferment'4 a mash consisting of the liquor resultant m the cooking of brous plant material with a solution-containing caustic alkali and an alkaiine sulphite until vthe brous plant material is softened but not pulped, and thereby producing reconstable distillable spirits. i

2. The process of manufacturing distillable spirits by fermentation which process com rises preparin a' mash consisting 'solel. o the liquorre tant from the' cooking of nbrous plant material with a solution containing caustic alkali and 'an alkaline sulphi until the fibrous plant material is softcned but vnot pulped adding water to said liquor, slightly acidil g the mixture prior to addition of the ferment to counteract normal alkalinity of the cookin men the mash so prepa producing recoverable distillable spirits.

3. The process of manufacturing distillable spirits by fermentation which process comp'rises fermentinga mash consisting of a liquor resultant from the cookingv of fibrous plant material with mild cooking agents includin in solution caustic alkali and an alkali uor ,ferand therebyline su phur compound until the fibrous plant material is softened butA not ulped, and said liquor includin hemi-cellulbses, pentosans, albuminous an mucilaginous matter, and thereby producing recoverable distillable spirits.

4. The process of manufacturing distll` able spirits by fermentation -which process comprises fermenting a mash consisting of the hquor resulting from washing fibrous plant material after the same has been cooked with a mild cooking agent comprising a solution containin` caustic alkali and an alkalm e sulphite, s ightly acidifyin the liquor prior to the incorporation of t e ferment, fermentin the mash so prepared and thereby producing recoverable distillable spirits.

5. The process of manufacturing distillable spirits by fermentation which process comprises fermenting a mash consisting solely of the liquor resultant from the -cooking of fibrous plant material with a mild cooking aglent comprising a solution of sodium sul- P ite containing caustic soda until the fibrous plant material is softened but not pulped, and thereby producing recoverable distillable spirits.

6. The process of manufacturing chemicals by fermentation'which process consists of preparing a culture of a micro-organism in an amount of the liquor resultant from the cookin of fibrous plant material with a mild coo 'ng agent including' in solution sodium sulphite and caustic alkali ,until the fibrous plant material is softened but not pulped, incorporating the culture in a largeamount of the same kind of liquor and permitting fermentation to take place, and thereby producing recoverable distillable spirits.

7. The process of manufacturing distillable spirits by fermentation which process comprises fermenting a mash consisting of the liquor resultant from the cooking of iibrous plant material with a solution of caustic soda and an alkaline sulphur compound until the fibrous plant material is softened but not pulped, and thereby producing recoverable distillable spirits.

'8. The process of manufacturing distillable spirits by fermentation which' process comprises fermenting amash consisting of the f but not pulped, and thereby producing recoverable distillable spirits.

9. The process of manufacturing distillable spirits by fermentation which recess consists of fermenting a mash comprising the liquor resultant from the cooking of fibrous plant material with a. mild cooking agent comprising a Weak solutionof a caustic alkali and. which cooking is conducted until the brous plant material is softened but not pulped, and thereby producing recoverable distillable spirits.

10. The process of manufacturing alcohol by fermentation Whichprocess comprises fermenting a mash comprising the liquor resultant from the cooking of fibrous plant material with a solution of a caustic alkali, and thereby recovering distillable spirits.

11. The process of manufacturing alcohol by fermentation. which process consists in fermenting with a micro-organism a mash comprising the liquor resultant of the cooking of fibrous plant material with alkaline hydroxide, and recovering the distillable spirits produced.

' 12. The process of manufacturing alcohol by fermentation which process consists in fermenting with a micro-organism a mash comprising the liquor resultant of the cook` ing of fibrous plant material with sodium hydroxide, and recovering the .distillable spirits produced.

ln testimony whereof l aiiix my signature.

SIDNEY D. WELLSn 

